CN102690111A - Nickel-copper-zinc soft magnetic ferrite material for low temperature co-firing and preparation method thereof - Google Patents
Nickel-copper-zinc soft magnetic ferrite material for low temperature co-firing and preparation method thereof Download PDFInfo
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- CN102690111A CN102690111A CN2012101197925A CN201210119792A CN102690111A CN 102690111 A CN102690111 A CN 102690111A CN 2012101197925 A CN2012101197925 A CN 2012101197925A CN 201210119792 A CN201210119792 A CN 201210119792A CN 102690111 A CN102690111 A CN 102690111A
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Abstract
The invention, pertaining to a field of a soft magnetic ferrite material, particularly relates to a nickel-copper-zinc soft magnetic ferrite material for low temperature co-firing, comprising principal constituents and auxiliary constituents. The principal constituents comprise iron oxide, nickel oxide, zinc oxide and cupric oxide. The contents of the principal constituents are 45.5 to 49.5 mol% of Fe2O3, 18.5 to 20.5 mol% of NiO, 24.0 to 28.5 mol% of ZnO and 6.0 to 8.0 mol% of CuO. The auxiliary constituents comprise manganese oxides and bismuth oxide. With respect to the gross of the principal components, the total content of the auxiliary constituents calculated by respective reference substances of MnO and Bi2O3 is 1.1wt% to 3.5wt%. The invention further provides a preparation method of the ferrite material. The material of the invention is used for preparing an MLCI device which is used under high frequency, has a comparatively low sintering temperature to ensure that metallic silver is not likely to spread in co-firing, and guarantees the MLCI device to obtain excellent magnetic characteristics and good consistency.
Description
Technical field
The invention belongs to the soft magnetic ferrite field, be specifically related to a kind of low temperature co-fired with ambrose alloy Zn soft magnetic ferrite material and preparation method thereof.
Background technology
Along with the mobile communication technology and the continual renovation replacements wired, the wireless digital communication net such as notebook computer, panel computer, smart mobile phones, electronic product is towards miniaturized, the develop rapidly of portability direction.This drives the emergence of surface mounting technique (SMT).The SMC slice component can not only make miniaturization of electronic products, and can realize the high-speed automated of final assembly, the widespread use of slice component, and manufacturers hopes that printed substrate all adopts slice component.Over the past two decades; The resistor in the three big passive elements and the chip type technical development of electrical condenser are very rapidly; Product category and specification are complete day by day; Reached the high volume applications stage, and miniaturized chip magnetics (comprising inducer, magnetic bead, wave filter, Microwave Iron Oxide Elements etc.) is because technology difficulty is bigger, so development is slow relatively.Some countries drop into the chip type technology that a large amount of manpower financial capacities research and develop magnetics in recent years, thereby effectively promote the development of miniaturized chip magnetics.Maturation along with Technologies such as lamination-type chip magnetic bead MLCB, laminated chip inductor MLCI; The communication in modern times of miniaturized chip magnetics, computingmachine, audio-visual equipment, teleworking equipment, automobile electronic system, military electronic installation and electromagnetic compatibility fields such as (EMC) have obtained using widely; Annual with double-digit speed increment, become one of most important electronic element.One of gordian technique of preparation MLCI and MLCB is the high-performance low-temperature sintered ferrite powder of preparation.Low-temperature sintering NiCuZn powder best on the our times is provided by Japanese TDK, field, village etc., and these companies carry out blockade on new techniques to China, do not sell its powder.The ferrite magnetic powder that is used to make chip ferrite elements such as laminated chip inductor, lamination sheet type ferrite bean and LC wave filter and compound multichip module (MCM) must possess following characteristic: 1) can low-temperature sintering.When the following temperature sintering of the fusing point (910 ℃) of inner wire Ag, can obtain fine and close ferrite microtexture and good electromagnetic performance.2) can burn altogether with the Ag slurry.When about 900 ℃, burning altogether with Ag slurry, with Ag chemical reaction not taking place, Ag ion diffusion phenomenon do not occur.3) satisfy the requirement of curtain coating, typography, the size-grade distribution of powder, pattern, surface characteristic etc. adapt to the requirement of curtain coating, typography.4) satisfy three layers of depositing process requirement, process ML and MLCB with magnetic after, its surface property can adapt to the condition of three layers of plating of end electrode, and the variation behind big direct current electrode position of its electromagnetic performance is little.
Publication number is the Chinese invention patent of CN101236819A; A kind of nickel-copper-zinc ferrite and method of manufacture thereof are provided; This ferrite comprises principal constituent and minor component; Principal constituent is not for being: red stone, nickel protoxide, zinc oxide, cupric oxide, and said principal constituent is following in the content of standard substance separately, Fe
2O
3: 48mol%～50 mol %, NiO:13 mol %～16 mol %, ZnO:29 mol %～31.5 mol %, CuO:4.5 mol %～6.5 mol %; Said minor component comprises vanadium oxide, molybdenum oxide, titanium oxide, said relatively principal constituent total amount, and said minor component is with its standard substance V separately
2O
5, MOO
3, TIO
2The total content of meter is 0.01wt%～0.08wt%.But this invention exists substance different with technical scheme of the present invention, and the material property that provides also has very big difference.
Summary of the invention
The object of the invention at first provides a kind of low temperature co-fired ambrose alloy Zn soft magnetic ferrite material of using, and second purpose provides the preparation method of described Ferrite Material.
For realizing the object of the invention, the contriver provides following technical proposals:
A kind of low temperature co-fired ambrose alloy Zn soft magnetic ferrite material of using is made up of principal constituent and minor component, and wherein, described principal constituent comprises red stone, nickel oxide, zinc oxide and cupric oxide, and principal constituent with mole percent level separately is: Fe
2O
3: 45.5～49.5mol%, NiO:18.5～20.5mol%, ZnO:24.0～28.5mol%, CuO:6.0～8.0mol%; Said minor component comprises the oxide compound and the bismuth oxide of manganese, and with respect to described principal constituent gross weight, said minor component is with its standard substance MnO and Bi
2O
3The weight percent total amount of meter is 1.1～3.5wt%.
The contriver finds through lot of experiments, through reasonable control ferrite principal constituent proportioning, especially controls Fe
2O
3With the content of ZnO and be equipped with suitable minor component, can obtain that a kind of (1MHz～60MHz) has higher magnetic permcability μ i, high Q value during work, hangs down than temperature factor α μ at high frequency
r, characteristic such as high-curie temperature Tc and high Bs, high direct current biasing, anti-rush of current ambrose alloy Zn soft magnetic ferrite magnetic; Be used to prepare chip multilayer inducer (MLCI) device that uses under the high frequency, particularly under 1MHz～10MHz, have high Q value and low ratio temperature system.
In the above-mentioned principal constituent scope, if Fe
2O
3Content then can not get desirable high saturation magnetic flux density Bs less than 45.5mol%; If Fe
2O
3Content is greater than 49.5mol%, then the Q value reduce, than temperature factor α μ
rIncrease, can not get desirable magnetic core low loss characteristic.If ZnO content is less than 24mol%, then magnetic permeability descends; If ZnO content is greater than 28.5mol%, then the material Tc reduces, and saturation magnetic flux density Bs descends.
Above-mentioned minor component mainly is to form resistive formation at the ferrite crystal boundary, and the work of a fusing assistant is in order to reduce sintering temperature.When their content is lower than lower value, 910 ℃ of the sintering temperatures (> of the resistivity decreased of material or needs raising material); And when their content is higher than above-mentioned higher limit, then cause crystal grain misgrowth easily, core loss is worsened.
As preferably; According to a kind of low temperature co-fired ambrose alloy Zn soft magnetic ferrite material of using of the present invention, wherein, with respect to described principal constituent gross weight; The oxide compound of described minor component manganese and bismuth oxide in the weight percent content of standard substance separately are: MnO:0.1～0.50wt%, Bi
2O
3: 1.0～3.0wt%.
As preferably, according to a kind of low temperature co-fired ambrose alloy Zn soft magnetic ferrite material of using of the present invention, wherein, described minor component further comprises Co
2O
3, V
2O
5, ZrO
2, SiO
2In one or more, with respect to described principal constituent gross weight, these minor components in the weight percent content of its standard substance are: Co
2O
3: 0.05～1.0wt%, V
2O
5: 0.05～0.50wt%, ZrO
2: 0～0.5wt%, SiO
2: 0.05～1.0wt%.
Above-mentioned minor component mainly can reduce ferritic magnetic hysteresis loss, crystal grain thinning to improve the high frequency Q value of material.When their content was lower than lower value, the Q value of material descended; And when their content is higher than above-mentioned higher limit, then cause crystal grain misgrowth easily, core loss is worsened.
The present invention also provides above-mentioned a kind of low temperature co-fired preparation method with the ambrose alloy Zn soft magnetic ferrite material, comprises the steps: successively
(1) with principal constituent mixing, vibration, carries out pre-burning in the kiln of dropping a hint then, obtain preburning powdered material through initial reaction;
(2) preburning powdered material is carried out coarse reduction, add the minor component vibration, add sticker then and dry granulation, the particulate median size that obtains is at 1～15 μ m, water cut < 0.3wt%;
(3) adopt casting technique to prepare ferrite blank, sintering in 830～910 ℃ air kiln, soaking time is 120～180 minutes, obtains the described low temperature co-fired ambrose alloy Zn soft magnetic ferrite material of using.
As preferably, according to a kind of low temperature co-fired preparation method with the ambrose alloy Zn soft magnetic ferrite material of the present invention, wherein, calcined temperature is 750～850 ℃ in the described step (1), and soaking time is 120～180 minutes.
As preferably, according to a kind of low temperature co-fired preparation method with the ambrose alloy Zn soft magnetic ferrite material of the present invention, wherein, the oxide compound of minor component manganese is with Mn in the described step (2)
3O
4Form add.
As preferably; According to a kind of low temperature co-fired preparation method of the present invention with the ambrose alloy Zn soft magnetic ferrite material; Wherein, Dry method or wet processing are adopted in coarse reduction in the described step (2), and dry process adopts vibrating ball mill directly to pulverize, and wet processing is pulverized through ball mill or sand mill and carried out drying treatment then.
As preferably, according to a kind of low temperature co-fired preparation method with the ambrose alloy Zn soft magnetic ferrite material of the present invention, wherein, 60～120 minutes pulverizing time of described coarse reduction, the particulate median size that obtains is at 1～15 μ m.
Adopt casting technique to prepare the technology that ferrite blank refers to preparation lamination-type chip magnetic bead MLCB, laminated chip inductor MLCI employing in the above-mentioned step (3); Generally magnetic directly is pressed into standard toroidal core φ 25 * φ 15 * 5 during the test material characteristic, then it is inserted 830～910 ℃ of following sintering.
The present invention forms and content through control material principal constituent, minor component, especially controls Fe
2O
3, ZnO content and well-designed minor component prescription, optimize to add oxide compound and control pre-sinter process and sintering process, under existing manufacturing technique equipment, obtained comparatively ideal microtexture and material behavior with leading level in the world.Provided by the present invention low temperature co-firedly possess following properties with the ambrose alloy Zn soft magnetic ferrite material::
Magnetic permeability (μ i:40～60, f=1MHz);
The Q value (＞120,10MHz);
Than temperature system α μ ir (* 10
-6/ ℃):＜45 (55～25 ℃),＜30 (25～85 ℃);
Saturation induction density Bs (mT): 420 (4KA/m);
Tc Tc (℃):＞250.
Among the present invention, if no special instructions, the technical term of appearance or noun, its implication is the implication of the common indication in this area.
Compared with prior art, the invention has the beneficial effects as follows:
The present invention through well-designed material prescription and mix an amount of additive, a kind of high frequency (ambrose alloy Zn soft magnetic ferrite magnetic of chip multilayer inducer (MLCI) device of 1MHz～60MHz) use down that is used to prepare is provided.Utilize current production devices just can obtain to produce in batches, each characteristic of material is in international most advanced level.
The present invention adopts general soft magnetic ferrite dry preparation process, and its preparation technology is simple, cost of manufacture is low.Have lower sintering temperature, argent is difficult for diffusion when burning altogether; Can guarantee that chip multilayer inducer (MLCI) device obtains excellent magnetic properties, consistence is better.
The major and minor starting material of the present invention are chosen rationally, all adopt conventional starting material to make.
Embodiment
Below in conjunction with embodiment, content of the present invention is described more specifically.Should be appreciated that enforcement of the present invention is not limited to following embodiment, all will fall into protection domain of the present invention any pro forma accommodation and/or the change that the present invention made.
In the present invention, if not refer in particular to, all part, per-cents are weight unit, and all equipment and raw material etc. all can be buied from market or the industry is commonly used.
Embodiment 1
Principal constituent content with shown in the table 1 takes by weighing Fe
2O
3, NiO, ZnO and CuO starting material carry out dry mixed and vibration, pre-burning 120 minutes in 800 ℃ air kiln then obtains the preburning powdered material through initial reaction.In preburning powdered material weight, (with respect to described principal constituent gross weight, described minor component in the weight percent content of standard substance separately is: the MnO of 0.3wt%, the Bi of 2.5wt% in preburning powdered material, to add an amount of minor component
2O
3, 0.5wt% Co
2O
3, 0.05wt% V
2O
5, 0.1wt% ZrO
2, 0.3wt% SiO
2, the oxide compound of manganese is with Mn
3O
4Form add), sand milling 60 minutes, the particulate median size that obtains adds the sticker Z 150PH of 0.8wt% then and dries granulation at 10 μ m, the median size of the particle powder that obtains is in 12 μ m, water cut<0.3wt% adopts casting technique that powder is pressed into standard ring blank φ 25 * φ 15 * 5, then it is inserted sintering 880 times, and soaking time 2 hours obtains the described low temperature co-fired ambrose alloy Zn soft magnetic ferrite material of using.
Adopt the HP4291B instrument at U=0.5V, N=20T
S, T=25 ℃ of magnetic permeability μ i that detects down magnetic, Q value, than temperature factor α μ r, Tc Tc; Adopt the SY8258 appearance at H=4KA/m, test saturation induction density Bs down for T=25 ℃; Adopt MS 8220 appearance at U=500V, T=25 ℃ of following test surfaces resistance R.The result sees table 1.
Table 1
Find out from table 1, principal constituent content within the scope of the present invention, the saturation magnetic flux density of magnetic permeability μ i, magnetic core, Q value, than better performances such as temperature factor α μ r, Tc Tc.When main formula departs from the present invention, then exist saturation magnetic flux density reduce, than one or a few the tendencies that performance descends simultaneously in temperature factor α μ r increase, surface resistivity and the Q value etc.
Embodiment 2
The preparation technology of magnetic core is identical with embodiment 1.Fe during just principal constituent is filled a prescription
2O
3, NiO, ZnO, CuO content be fixed as the Fe of 47.5mol%
2O
3, the NiO of 19.5mol%, the ZnO of 26.0mol% and the CuO of 7.0mol%.The content of minor component is as shown in table 2.
Table 2
Continuous table 2
Can find out from table 2, when the content of minor component within the scope of the present invention, the saturation magnetic flux density of magnetic permeability μ i, magnetic core, Q value, than better performances such as temperature factor α μ r, Tc Tc.When main formula departs from the present invention, then exist saturation magnetic flux density reduce, than one or a few the tendencies that performance descends simultaneously in temperature factor α μ r increase, surface resistivity and the Q value etc.
Embodiment 3
The composition of magnetic core is identical with test number 104#, and preparation technology is identical with embodiment 1.Just calcined temperature is as shown in table 3.
Table 3
Can find out from table 3, when calcined temperature is in the present invention, the saturation magnetic flux density of magnetic permeability μ i, magnetic core, Q value, than better performances such as temperature factor α μ r, Tc Tc.Be lower than and when being higher than 750～850 ℃, then exist saturation magnetic flux density reduce, than one or a few the tendencies that performance descends simultaneously in temperature factor α μ r increase, surface resistivity and the Q value etc.
Embodiment 4
The composition of magnetic core is identical with test number 104#, and preparation technology is identical with embodiment 1.Just sintering temperature is as shown in table 4.
Table 4
Can find out from table 4, when sintering temperature is in the present invention, the saturation magnetic flux density of magnetic permeability μ i, magnetic core, Q value, than better performances such as temperature factor α μ r, Tc Tc.When being lower than 830 ℃, then there are one or a few the tendencies that performance descends simultaneously in magnetic permeability μ i, the saturation magnetic flux density reduction etc.; When sintering temperature is higher than 910 ℃, Ag ion diffusion phenomenon will appear in the lamination-type chip magnetic bead MLCB, the laminated chip inductor MLCI that prepare with casting technique.
The foregoing description just is used for explanation and explains content of the present invention can not constituting limitation of the scope of the invention.Although the contriver has done in more detail the present invention and has enumerated; But; The content that those skilled in the art is disclosed according to summary of the invention part and embodiment; Can make various modifications or/and to replenish or adopt similar mode to substitute be obvious to described specific embodiment, the term that occurs among the present invention is used for can not being construed as limiting the invention the elaboration of technical scheme of the present invention and understanding.
Claims (8)
1. the low temperature co-fired ambrose alloy Zn soft magnetic ferrite material of using is formed and is comprised principal constituent and minor component, it is characterized in that described principal constituent comprises red stone, nickel oxide, zinc oxide and cupric oxide, and principal constituent with mole percent level separately is: Fe
2O
3: 45.5～49.5mol%, NiO:18.5～20.5mol%, ZnO:24.0～28.5mol%, CuO:6.0～8.0mol%; Described minor component comprises the oxide compound and the bismuth oxide of manganese, and with respect to described principal constituent gross weight, described minor component is with its standard substance MnO and Bi
2O
3The weight percent total amount of meter is 1.1～3.5wt%.
2. a kind of low temperature co-fired ambrose alloy Zn soft magnetic ferrite material of using as claimed in claim 1; It is characterized in that; With respect to described principal constituent gross weight, the oxide compound of described minor component manganese and bismuth oxide in the weight percent content of standard substance separately are: MnO:0.1～0.50wt%, Bi
2O
3: 1.0～3.0wt%.
3. a kind of low temperature co-fired ambrose alloy Zn soft magnetic ferrite material of using as claimed in claim 1 is characterized in that described minor component further comprises Co
2O
3, V
2O
5, ZrO
2, SiO
2In one or more, with respect to described principal constituent gross weight, these minor components in the weight percent content of its standard substance are: Co
2O
3: 0.05～1.0wt%, V
2O
5: 0.05～0.50wt%, ZrO
2: 0～0.5wt%, SiO
2: 0.05～1.0wt%.
4. the described a kind of low temperature co-fired preparation method with the ambrose alloy Zn soft magnetic ferrite material of one of claim 1-3 is characterized in that described preparation method comprises the steps: successively
(1) with principal constituent mixing, vibration, carries out pre-burning in the kiln of dropping a hint then, obtain preburning powdered material through initial reaction;
(2) preburning powdered material is carried out coarse reduction, add the minor component vibration, add sticker then and dry granulation, the particulate median size that obtains is at 1～15 μ m, water cut < 0.3wt%;
(3) adopt casting technique to prepare ferrite blank, sintering in 830～910 ℃ air kiln, soaking time is 120～180 minutes, obtains the described low temperature co-fired ambrose alloy Zn soft magnetic ferrite material of using.
5. a kind of low temperature co-fired preparation method with the ambrose alloy Zn soft magnetic ferrite material according to claim 4 is characterized in that, calcined temperature is 750～850 ℃ in the described step (1), and soaking time is 120～180 minutes.
6. a kind of low temperature co-fired preparation method with the ambrose alloy Zn soft magnetic ferrite material according to claim 4 is characterized in that, the oxide compound of minor component manganese is with Mn in the described step (2)
3O
4Form add.
7. a kind of low temperature co-fired preparation method according to claim 4 with the ambrose alloy Zn soft magnetic ferrite material; It is characterized in that; Dry method or wet processing are adopted in coarse reduction in the described step (2); Dry process adopts vibrating ball mill directly to pulverize, and wet processing is pulverized through ball mill or sand mill and carried out drying treatment then.
8. a kind of low temperature co-fired preparation method with the ambrose alloy Zn soft magnetic ferrite material according to claim 4 is characterized in that 60～120 minutes pulverizing time of described coarse reduction, the particulate median size that obtains is at 1～15 μ m.
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| CN102807361A (en) * | 2012-07-03 | 2012-12-05 | 天通控股股份有限公司 | Nickel-zinc ferrite material for wireless signal sensing, sheet core and preparation method thereof |
| CN103332928A (en) * | 2012-11-02 | 2013-10-02 | 横店集团东磁股份有限公司 | Soft-magnetic nickel-copper-zinc ferrite material and preparation method thereof |
| CN104402424A (en) * | 2014-11-07 | 2015-03-11 | 乳源东阳光磁性材料有限公司 | Nickel-zinc ferrite material having high saturation magnetic flux density, high direct current superposition, and high Curie temperature, and preparation method thereof |
| CN109437878A (en) * | 2018-11-01 | 2019-03-08 | 沅陵辰州磁电高科有限公司 | Ni-Zn soft magnetic ferrite material |
| CN110041064A (en) * | 2019-04-17 | 2019-07-23 | 临沂成合信息技术有限公司 | Low temperature co-fired soft ferromagnetic powder of Stacked magnetic bead high impedance value and preparation method thereof |
| CN111792925A (en) * | 2020-07-23 | 2020-10-20 | 中国电子科技集团公司第九研究所 | High-magnetic-permeability wide-temperature-power type nickel-zinc LTCF material, and preparation method and application thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102807361A (en) * | 2012-07-03 | 2012-12-05 | 天通控股股份有限公司 | Nickel-zinc ferrite material for wireless signal sensing, sheet core and preparation method thereof |
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| CN103332928A (en) * | 2012-11-02 | 2013-10-02 | 横店集团东磁股份有限公司 | Soft-magnetic nickel-copper-zinc ferrite material and preparation method thereof |
| CN104402424A (en) * | 2014-11-07 | 2015-03-11 | 乳源东阳光磁性材料有限公司 | Nickel-zinc ferrite material having high saturation magnetic flux density, high direct current superposition, and high Curie temperature, and preparation method thereof |
| CN104402424B (en) * | 2014-11-07 | 2017-10-24 | 乳源东阳光磁性材料有限公司 | High saturation magnetic flux density, high DC stacked, high-curie temperature nickel-zinc-ferrite material and preparation method thereof |
| CN109437878A (en) * | 2018-11-01 | 2019-03-08 | 沅陵辰州磁电高科有限公司 | Ni-Zn soft magnetic ferrite material |
| CN110041064A (en) * | 2019-04-17 | 2019-07-23 | 临沂成合信息技术有限公司 | Low temperature co-fired soft ferromagnetic powder of Stacked magnetic bead high impedance value and preparation method thereof |
| CN111792925A (en) * | 2020-07-23 | 2020-10-20 | 中国电子科技集团公司第九研究所 | High-magnetic-permeability wide-temperature-power type nickel-zinc LTCF material, and preparation method and application thereof |
| CN111792925B (en) * | 2020-07-23 | 2022-12-02 | 中国电子科技集团公司第九研究所 | High-permeability wide-temperature-power type nickel-zinc LTCF material, and preparation method and application thereof |
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